CN102247811A - Preparation method and application of natural trass-sodium alginate composite microsphere water body purification material - Google Patents
Preparation method and application of natural trass-sodium alginate composite microsphere water body purification material Download PDFInfo
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Abstract
The invention provides a preparation method and application of a natural trass-sodium alginate composite microsphere water body purification material in the field of water body purification. In the preparation method, natural trass is dispersed in a sodium alginate solution to obtain a trass-sodium alginate suspension; the trass-sodium alginate suspension is dropwise added into a calcium chloride solution; and a trass-sodium alginate composite microsphere formed through crosslinking is dried or directly used as a water body purification material. The water body purification material prepared by the method can be effectively applied to adsorption and removal of phosphor in a water body, has the advantages of low cost, convenience in operation process, environmental friendliness, safety, easiness for mass production and the like, and can be widely applied to water body eutrophication control in the future.
Description
Technical field
What the present invention relates to is a kind of scavenging material and preparation and application of water body purification technical field, specifically is a kind of natural scoria-sodium alginate complex microsphere water body purification material preparation method and application thereof.
Background technology
As everyone knows, the discharging of China rural area sanitary sewage disperses, away from the blowdown pipe network, environmental capacity of water is little simultaneously, and the production, the sanitary wastewater that are rich in phosphorus in a large number generally directly enter rivers and lakes without any processing, are the primary pollution source that directly causes the natural water eutrophication.Therefore, how scientificlly and effectively control purifies China's phosphorous productive life sewage in rural area, has become the environmental problem that China needs to be resolved hurrily.
Based on the water body purification technology of function sorbing material, demonstrating its wide application prospect day by day aspect the control body eutrophication.As everyone knows, the active carbon porous material is widely used in water pollutant absorption and removes, recently, international environment field correlative study worker be entitled as " Phosphate removal by anion binding on functionalized nanoporous sorbents " (removing phosphate radical) based on the anionic functional nano adsorption material (" Environmental Science ﹠amp; Technology ", WILAIWAN CHOUYYOK, ROBERT J.WIACEK; KANDA PATTAMAKOMSAN et al, 2010, volume 44; page number 3073-3078) bibliographical information, research iron modification mesoporous silicon porous material effectively adsorbs the behavioral mechanism of removing phosphor contaminant.But it is worthy of note that the synthetic production cost of above-mentioned sorbing material is comparatively expensive.
Therefore, development provides high selectivity, water body with low cost, the environmental friendliness non-secondary pollution to control scavenging material, and for practical guarantee water resource safety, the protection people's health obviously has important actual social effect.
The natural scoria porous material that the domestic reserves in China Jilin Province are abundant, the a large amount of lava chips and the dust that erupt with syntectite when being volcanic eruption, be deposited on the material that forms loose or slight gluing in ground surface or the water, mainly contain elemental compositions such as inorganic silicon, oxygen, calcium, aluminium, iron, titanium in the structure, wherein calcium oxide, iron oxide, aluminium oxide, titanium oxide can be used as avtive spot, with the phosphate groups generation specificity combination that may exist in the water body, thereby effectively total phosphor contaminant in the water body is removed in absorption.But directly adsorb when removing in the water body total phosphor contaminant based on the natural scoria porous material, " muddy water " mixing phenomena can take place with Separation of Solid and Liquid difficulty between water body in the natural scoria porous material.
Summary of the invention
The present invention is directed to the prior art above shortcomings, a kind of natural scoria-sodium alginate complex microsphere water body purification material preparation method and application thereof is provided, with the natural high molecular substance sodium alginate is carrier, prepare natural scoria-sodium alginate complex microsphere by the calcium ion-exchanged process, make have the adsorption activity site the natural scoria porous material evenly parcel be distributed in mass-transfer performance good, have in the sodium alginate polymer microsphere of cross-linked structure.Based on this natural scoria-sodium alginate complex microsphere water body purification material, when being applied in the water body total phosphorus absorption and removing, effect is satisfied.
The present invention is achieved by the following technical solutions:
The present invention relates to a kind of natural scoria-sodium alginate complex microsphere water body purification preparation methods, obtain dropwise splashing in the calcium chloride solution behind scoria-sodium alginate suspension solution by natural scoria being scattered in sodium alginate soln, be cross-linked to form scoria-sodium alginate complex microsphere drying or directly as the water body purification material.
Described natural scoria is meant: through the scoria particle of vibration cleaning and heating, drying, its consumption is 0.5kg;
Described natural scoria through vibration cleaning and grain diameter is: below 200 orders.
The concentration of described sodium alginate soln is: 0.5～3.0wt%.
The concentration of described calcium chloride solution is: 0.05～1.50mol/L, its consumption are 200mL.
Described dispersion is meant: behind the ratio adding sodium alginate soln of natural scoria with 30-40g/1L, adopt magnetic stirrer evenly to stir and the ultrasonic air bubble of removing wherein.
Described drying is meant: scoria-sodium alginate complex microsphere tiling is placed electrically heated drying cabinet dry 20h under 70 ℃ of environment.
The chemical constituent that the present invention relates to natural scoria-sodium alginate complex microsphere water body purification material that method for preparing obtains is sodium alginate-supported body and volcanic ash, and its mass ratio is 1: 8～1: 1; Wherein the molecular formula of sodium alginate is (C
6H
7NaO
6) n, pozzuolanic constituent content (mass percent) is: Fe 8.81%, Al 8.89%, Ti 1.37%, Ca 4.91%, Mg3.19%, K 1.67%, Na 3.22%, Si 21.10% and O 46.84%.
Described scavenging material is the complex microsphere structure, and average grain diameter is 0.5～3.0mm.
The present invention relates to the purification method of above-mentioned natural scoria-sodium alginate complex microsphere water body purification material, remove phosphor contaminant in the water body by described water body purification material being added Yu Shuizhong absorption.
The present invention adds by reference ammonium molybdate spectrophotometry that phosphorus concentration mainly comprises to determine absorption property in the water body behind the water body purification material:
The adsorption reaction time influences the material adsorption effect: get in the potassium dihydrogen phosphate of certain mass water body purification material 15mg/L under certain volume, in pH=3, shaking table oscillating reactions, vibration rotating speed 200r/min, adsorption temp is 25 ℃, get supernatant liquid at set intervals and measure phosphorus concentration, draw the Changing Pattern of adsorption effect with adsorption time.
Water body purification material dosage is to the phosphorus Adsorption Effect: the potassium dihydrogen phosphate of 15mg/L of getting certain volume is in the polyethylene centrifuge tube, add the water body purification material of different quality respectively, in pH=3, shaking table oscillating reactions, vibration rotating speed 200r/min, adsorption temp is 25 ℃, the adsorption reaction time is 7h, measures solution supernatant phosphorus concentration after the reaction respectively, draws the Changing Pattern of adsorption effect with the material dosage.
Phosphorus solution under the different pH values influences the material adsorption effect: the water body purification material of getting certain mass adds respectively in the potassium dihydrogen phosphate of the 15mg/L of different pH values under the certain volume, the shaking table oscillating reactions, vibration rotating speed 200r/min, adsorption temp is 25 ℃, the adsorption reaction time is 7h, measure solution supernatant phosphorus concentration after the reaction respectively, draw the Changing Pattern of adsorption effect with the initial phosphorus solution pH of difference value.
Leave standstill the absorption of material under condition phosphorus effect: the water body purification material of getting certain mass adds in the potassium dihydrogen phosphate of 15mg/L of certain volume, leave standstill reaction, adsorption temp is 25 ℃, the adsorption reaction time is 7h, solution supernatant phosphorus concentration is measured in reaction back, draws under the condition of leaving standstill material to the adsorption effect of phosphorus in the water.
The preparation of this experiment phosphorus solution: take by weighing 0.0658 ± 0.001g with assay balance and analyze the pure phosphoric acid potassium dihydrogen, dissolving is dissolved in the 1000mL volumetric flask surely.
Description of drawings
The natural scoria that Fig. 1 prepares for the present invention-sodium alginate complex microsphere pattern characterizes Electronic Speculum figure.
Fig. 2 characterizes Electronic Speculum figure for the original pattern of the used natural scoria porous material of the present invention.
The specific embodiment
Below embodiments of the invention are elaborated, present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
(1) natural scoria preprocessing process:
Take by weighing the regional natural scoria 0.5kg in Huinan, Jilin Province, place deionized water, after abundant vibration is cleaned, drain to be placed on and dry 5h in the electrically heated drying cabinet under 100 ℃, back mechanical crushing, it is standby to cross 200 mesh sieves.
(2) preparation 2.0% sodium alginate soln (mass percent):
In glass beaker, add the 500mL deionized water in advance, be placed on the electric mixer, under 50 ℃ of heating conditions, pour the 10.0g sodium alginate solid that is taken by weighing fast into, be stirred well to this solution clear with the 500r/min rotating speed, the air bubble that may exist in the solution is removed with 100% power ultrasonic 3min in the back.
(3) preparation of 0.2mol/L calcium chloride solution:
Accurately take by weighing 22.198g anhydrous calcium chloride solid in the 500mL glass beaker, add after an amount of secondary deionized water fully dissolves, being transferred to 1000mL volumetric flask constant volume, to obtain the 0.2mol/L calcium chloride solution standby.
(4) preparation scoria-sodium alginate suspension (scoria mass percent 3.77%, sodium alginate mass percent 1.89%):
Take by weighing pretreated scoria powder among the 8.0g (1), be added in 2.0% sodium alginate soln of being prepared among the 200mL (2), make that scoria and sodium alginate mass percent are respectively in the solution: 3.77%, 1.89%.After this mixed solution is placed on the magnetic stirrer, with the full and uniform stirring of high speed 30min, it is standby to obtain scoria-sodium alginate suspension.
(5) be cross-linked to form scoria-sodium alginate complex microsphere:
After prepared suspension is removed the air bubble that wherein may exist with 100% power ultrasonic 3min in (4), scoria-sodium alginate suspension is passed through peristaltic pump, under the 2mL/min flow velocity, dropwise splash into (this solution places the 500mL glass beaker) in the 200mL 0.2mol/L calcium chloride solution, the scoria-sodium alginate micro ball that is cross-linked to form is dispersed in the 500mL glass beaker.After make microballoon in former calcium chloride solution, leave standstill 12h so that this micro-sphere crosslinked reacting completely, with washed with de-ionized water thus obtained microsphere 3 times, be neutrality to the supernatant cleaning fluid after, the absorption that is directly used in phosphorus in the water after the filtration is removed.
(6) the moisture natural scoria-sodium alginate complex microsphere for preparing, as effective water body purification material, the absorption that is applied to phosphorus in the water is removed:
The chemical constituent of the moisture natural scoria that present embodiment prepares-sodium alginate complex microsphere water body purification material is sodium alginate-supported body, volcanic ash and water; Wherein the molecular formula of sodium alginate is (C
6H
7NaO
6) n, pozzuolanic constituent content (mass percent) is: Fe 8.81%, Al 8.89%, Ti 1.37%, Ca 4.91%, Mg3.19%, K 1.67%, Na 3.22%, Si 21.10% and O 46.84%.The average grain diameter of prepared natural scoria-sodium alginate complex microsphere is 3.0mm.
Experiment is removed in the phosphorus absorption in water of prepared water body purification material application, test draws, and is in the 15mg/L potassium dihydrogen phosphate, at pH=3 in that the 8.0g material is dropped into the 10mL initial concentration, be oscillating reactions 7h on the shaking table of 200r/min at rotating speed, the clearance of phosphorus is 92.67%; Simultaneously, the static reaction clearance is 90.82% under the same conditions.
Embodiment 2
(1) natural scoria preprocessing process:
Take by weighing the regional natural scoria 0.5kg in Huinan, Jilin Province, place deionized water, after abundant vibration is cleaned, drain to be placed on and dry 5h in the electrically heated drying cabinet under 100 ℃, back mechanical crushing, it is standby to cross 200 mesh sieves.
(2) preparation 0.5% sodium alginate soln (mass percent):
In glass beaker, add the 500mL deionized water in advance, be placed on the electric mixer, under 50 ℃ of heating conditions, pour the 2.5g sodium alginate solid that is taken by weighing fast into, be stirred well to this solution clear with the 500r/min rotating speed, the air bubble that may exist in the solution is removed with 100% power ultrasonic 3min in the back.
(3) preparation of 0.05mol/L calcium chloride solution:
Accurately take by weighing 5.549g anhydrous calcium chloride solid in the 100mL glass beaker, add after an amount of secondary deionized water fully dissolves, being transferred to 1000mL volumetric flask constant volume, to obtain the 0.05mol/L calcium chloride solution standby.
(4) preparation scoria-sodium alginate suspension (scoria mass percent 2.90%, sodium alginate mass percent 0.48%):
Take by weighing pretreated scoria powder among the 6.0g (1), be added in 0.5% sodium alginate soln of being prepared among the 200mL (2), make that scoria and sodium alginate mass percent are respectively in the solution: 2.90%, 0.48%.After this mixed solution is placed on the magnetic stirrer, with the full and uniform stirring of high speed 30min, it is standby to obtain scoria-sodium alginate suspension.
(5) be cross-linked to form scoria-sodium alginate complex microsphere:
After prepared suspension is removed the air bubble that wherein may exist with 100% power ultrasonic 3min in (4), scoria-sodium alginate suspension is passed through peristaltic pump, under the 2mL/min flow velocity, dropwise splash into (this solution places the 500mL glass beaker) in the 200mL 0.05mol/L calcium chloride solution, the scoria-sodium alginate micro ball that is cross-linked to form is dispersed in the 500mL glass beaker.After make microballoon in former calcium chloride solution, leave standstill 12h so that this micro-sphere crosslinked reacting completely, with washed with de-ionized water thus obtained microsphere 3 times, be neutrality to the supernatant cleaning fluid after, filter standby.
(6) the dry scoria-sodium alginate complex microsphere of handling:
Place electrically heated drying cabinet, temperature to be set to 70 ℃ thus obtained microsphere tiling in above-mentioned (5), drying time, 20h made the complete dehydration of wet microballoon, and obtaining dry average grain diameter is scoria-sodium alginate complex microsphere of 0.5～1.0mm.
(7) the dry natural scoria-sodium alginate complex microsphere for preparing, as effective water body purification material, the absorption that is applied to phosphorus in the water is removed:
The chemical constituent of the natural scoria that present embodiment prepares-sodium alginate complex microsphere water body purification material is sodium alginate-supported body and volcanic ash, and its mass ratio is 1: 6; Wherein the molecular formula of sodium alginate is (C
6H
7NaO
6) n, pozzuolanic constituent content (mass percent) is: Fe 8.81%, Al 8.89%, Ti 1.37%, Ca 4.91%, Mg3.19%, K 1.67%, Na 3.22%, Si 21.10% and O 46.84%.The average grain diameter of prepared natural scoria-sodium alginate complex microsphere is 0.5～1.0mm.Prepared material natural scoria-sodium alginate complex microsphere pattern characterizes sees accompanying drawing 1.
Experiment is removed in the phosphorus absorption in water of prepared water body purification material application, test draws, and is in the 15mg/L potassium dihydrogen phosphate, at pH=3 in that the 3.0g material is dropped into the 10mL initial concentration, be oscillating reactions 7h on the shaking table of 200r/min at rotating speed, the clearance of phosphorus is 89.37%; Simultaneously, the static reaction clearance is 72.80% under the same conditions.
Embodiment 3
(1) natural scoria preprocessing process:
Take by weighing the regional natural scoria 0.5kg in Huinan, Jilin Province, place deionized water, after abundant vibration is cleaned, drain to be placed on and dry 5h in the electrically heated drying cabinet under 100 ℃, back mechanical crushing, it is standby to cross 200 mesh sieves.
(2) preparation 2.0% sodium alginate soln (mass percent):
In glass beaker, add the 500mL deionized water in advance, be placed on the electric mixer, under 50 ℃ of heating conditions, pour the 10.0g sodium alginate solid that is taken by weighing fast into, be stirred well to this solution clear with the 500r/min rotating speed, the air bubble that may exist in the solution is removed with 100% power ultrasonic 3min in the back.
(3) preparation of 0.2mol/L calcium chloride solution:
Accurately take by weighing 22.198g anhydrous calcium chloride solid in the 500mL glass beaker, add after an amount of secondary deionized water fully dissolves, being transferred to 1000mL volumetric flask constant volume, to obtain the 0.2mol/L calcium chloride solution standby.
(4) preparation scoria-sodium alginate suspension (scoria mass percent 3.77%, sodium alginate mass percent 1.89%):
Take by weighing pretreated scoria powder among the 8.0g (1), be added in 2.0% sodium alginate soln of being prepared among the 200mL (2), make that scoria and sodium alginate mass percent are respectively in the solution: 3.77%, 1.89%.After this mixed solution is placed on the magnetic stirrer, with the full and uniform stirring of high speed 30min, it is standby to obtain scoria-sodium alginate suspension.
(5) be cross-linked to form scoria-sodium alginate complex microsphere:
After prepared suspension is removed the air bubble that wherein may exist with 100% power ultrasonic 3min in (4), scoria-sodium alginate suspension is passed through peristaltic pump, under the 2mL/min flow velocity, dropwise splash into (this solution places the 500mL glass beaker) in the 200mL 0.2mol/L calcium chloride solution, the scoria-sodium alginate micro ball that is cross-linked to form is dispersed in the 500mL glass beaker.After make microballoon in former calcium chloride solution, leave standstill 12h so that this micro-sphere crosslinked reacting completely, with washed with de-ionized water thus obtained microsphere 3 times, be neutrality to the supernatant cleaning fluid after, filter standby.
(6) the dry scoria-sodium alginate complex microsphere of handling:
Place electrically heated drying cabinet, temperature to be set to 70 ℃ thus obtained microsphere tiling in above-mentioned (5), drying time, 20h made the complete dehydration of wet microballoon, and obtaining dry average grain diameter is scoria-sodium alginate complex microsphere of 1.0mm.
(7) the dry natural scoria-sodium alginate complex microsphere for preparing, as effective water body purification material, the absorption that is applied to phosphorus in the water is removed:
The chemical constituent of the natural scoria that present embodiment prepares-sodium alginate complex microsphere water body purification material is sodium alginate-supported body and volcanic ash, and its mass ratio is 1: 2; Wherein the molecular formula of sodium alginate is (C
6H
7NaO
6) n, pozzuolanic constituent content (mass percent) is: Fe 8.81%, Al 8.89%, Ti 1.37%, Ca 4.91%, Mg3.19%, K 1.67%, Na 3.22%, Si 21.10% and O 46.84%.The average grain diameter of prepared natural scoria-sodium alginate complex microsphere is 1.0mm.Prepared material natural scoria-sodium alginate complex microsphere pattern characterizes sees accompanying drawing 1.
Experiment is removed in the phosphorus absorption in water of prepared water body purification material application, test draws, and is in the 15mg/L potassium dihydrogen phosphate, at pH=3 in that the 1.5g material is dropped into the 10mL initial concentration, be oscillating reactions 7h on the shaking table of 200r/min at rotating speed, the clearance of phosphorus is 98.31%; Simultaneously, the static reaction clearance is 94.80% under the same conditions.
Embodiment 4
(1) natural scoria preprocessing process:
Take by weighing the regional natural scoria 0.5kg in Huinan, Jilin Province, place deionized water, after abundant vibration is cleaned, drain to be placed on and dry 5h in the electrically heated drying cabinet under 100 ℃, the back is by mechanical crushing, and it is standby to cross 200 mesh sieves.
(2) preparation 2.0% sodium alginate soln (mass percent):
In glass beaker, add the 500mL deionized water in advance, be placed on the temperature control electric mixer, under 50 ℃ of heating conditions, pour the 10.0g sodium alginate solid that is taken by weighing fast into, be stirred well to this solution clear with the 500r/min rotating speed, the air bubble that may exist in the solution is removed with 100% power ultrasonic 3min in the back.
(3) preparation of 0.2mol/L calcium chloride solution:
Accurately take by weighing 22.198g anhydrous calcium chloride solid in the 500mL glass beaker, add after an amount of secondary deionized water fully dissolves, being transferred to 1000mL volumetric flask constant volume, to obtain the 0.2mol/L calcium chloride solution standby.
(4) preparation scoria-sodium alginate suspension (scoria mass percent 2.86%, sodium alginate mass percent 1.90%):
Take by weighing pretreated scoria powder among the 6.0g (1), be added in 2.0% sodium alginate soln of being prepared among the 200mL (2), make that scoria and sodium alginate percentage by weight are respectively in the solution: 2.86%, 1.90%.After this mixed solution is placed on the magnetic stirrer, with the full and uniform stirring of high speed 30min, it is standby to obtain scoria-sodium alginate suspension.
(5) be cross-linked to form scoria-sodium alginate complex microsphere:
After prepared suspension is removed the air bubble that wherein may exist with 100% power ultrasonic 3min in (4), scoria-sodium alginate suspension is passed through peristaltic pump, under the 2mL/min flow velocity, dropwise splash into (this solution places the 500mL glass beaker) in the 200mL 0.2mol/L calcium chloride solution, the scoria-sodium alginate micro ball that is cross-linked to form is dispersed in the 500mL glass beaker.After make microballoon in former calcium chloride solution, leave standstill 12h so that this micro-sphere crosslinked reacting completely, with washed with de-ionized water thus obtained microsphere 3 times, be neutrality to the supernatant cleaning fluid after, filter standby.
(6) the dry scoria-sodium alginate complex microsphere of handling:
Place electrically heated drying cabinet, temperature to be set to 70 ℃ thus obtained microsphere tiling in above-mentioned (5), drying time, 20h made the complete dehydration of wet microballoon, and obtaining dry average grain diameter is scoria-sodium alginate complex microsphere of 1.0mm.
(7) the dry natural scoria-sodium alginate complex microsphere for preparing, as effective water body purification material, the absorption that is applied to phosphorus in the water is removed.
The chemical constituent of the natural scoria that present embodiment prepares-sodium alginate complex microsphere water body purification material is sodium alginate-supported body and volcanic ash, and its mass ratio is 2: 3; Wherein the molecular formula of sodium alginate is (C
6H
7NaO
6) n, pozzuolanic constituent content (mass percent) is: Fe 8.81%, Al 8.89%, Ti 1.37%, Ca 4.91%, Mg3.19%, K 1.67%, Na 3.22%, Si 21.10% and O 46.84%.The average grain diameter of prepared natural scoria-sodium alginate complex microsphere is 1.0mm.Prepared material natural scoria-sodium alginate complex microsphere pattern characterizes sees accompanying drawing 1.
Experiment is removed in the phosphorus absorption in water of prepared water body purification material application, test draws, and is in the 15mg/L potassium dihydrogen phosphate, at pH=3 in that the 3g material is dropped into the 10mL initial concentration, be oscillating reactions 7h on the shaking table of 200r/min at rotating speed, the clearance of phosphorus is 90.31%; Simultaneously, the static reaction clearance is 70.0% under the same conditions.
Embodiment 5
(1) natural scoria preprocessing process:
Take by weighing the regional natural scoria 0.5kg in Huinan, Jilin Province, place deionized water, after abundant vibration is cleaned, drain to be placed on and dry 5h in the electrically heated drying cabinet under 100 ℃, back mechanical crushing, it is standby to cross 200 mesh sieves.
(2) preparation 2.0% sodium alginate soln (mass percent):
In glass beaker, add the 500mL deionized water in advance, be placed on the electric mixer, under 50 ℃ of heating conditions, pour the 10.0g sodium alginate solid that is taken by weighing fast into, be stirred well to this solution clear with the 500r/min rotating speed, the air bubble that may exist in the solution is removed with 100% power ultrasonic 3min in the back.
(3) preparation of 0.5mol/L calcium chloride solution:
Accurately take by weighing 55.495g anhydrous calcium chloride solid in the 500mL glass beaker, add after an amount of secondary deionized water fully dissolves, being transferred to 1000mL volumetric flask constant volume, to obtain the 0.5mol/L calcium chloride solution standby.
(4) preparation scoria-sodium alginate suspension (scoria mass percent 3.77%, sodium alginate mass percent 1.89%):
Take by weighing pretreated scoria powder among the 8.0g (1), be added in 2.0% sodium alginate soln of being prepared among the 200mL (2), make that scoria and sodium alginate percentage by weight are respectively in the solution: 3.77%, 1.89%.After this mixed solution is placed on the magnetic stirrer, with the full and uniform stirring of high speed 30min, it is standby to obtain scoria-sodium alginate suspension.
(5) be cross-linked to form scoria-sodium alginate complex microsphere:
After prepared suspension is removed the air bubble that wherein may exist with 100% power ultrasonic 3min in (4), scoria-sodium alginate suspension is passed through peristaltic pump, under the 2mL/min flow velocity, dropwise splash into (this solution places the 500mL glass beaker) in the 200mL 0.5mol/L calcium chloride solution, the scoria-sodium alginate micro ball that is cross-linked to form is dispersed in the 500mL glass beaker.After make microballoon in former calcium chloride solution, leave standstill 12h so that this micro-sphere crosslinked reacting completely, with washed with de-ionized water thus obtained microsphere 3 times, be neutrality to the supernatant cleaning fluid after, filter standby.
(6) the dry scoria-sodium alginate complex microsphere of handling:
Place electrically heated drying cabinet, temperature to be set to 70 ℃ thus obtained microsphere tiling in above-mentioned (5), drying time, 20h made the complete dehydration of wet microballoon, and obtaining dry average grain diameter is scoria-sodium alginate complex microsphere of 1.0mm.
(7) the dry natural scoria-sodium alginate complex microsphere for preparing, as effective water body purification material, the absorption that is applied to phosphorus in the water is removed:
The chemical constituent of the natural scoria that present embodiment prepares-sodium alginate complex microsphere water body purification material is sodium alginate-supported body and volcanic ash, and its mass ratio is 1: 2; Wherein the molecular formula of sodium alginate is (C
6H
7NaO
6) n, pozzuolanic constituent content (mass percent) is: Fe 8.81%, Al 8.89%, Ti 1.37%, Ca 4.91%, Mg3.19%, K 1.67%, Na 3.22%, Si 21.10% and O 46.84%.The average grain diameter of prepared natural scoria-sodium alginate complex microsphere is 1.0mm.Prepared material natural scoria-sodium alginate complex microsphere pattern characterizes sees accompanying drawing 1.
Prepared water body purification material is applied to phosphorus absorption removal in the water, and it is in the 15mg/L potassium dihydrogen phosphate that the 1.5g material is dropped into the 10mL initial concentration, and when pH=3,200r/min oscillating reactions 7h, tp removal rate are 97.89%; The static reaction clearance is 94.59% under the same terms.
Embodiment 6
(1) natural scoria preprocessing process:
Take by weighing the regional natural scoria 0.5kg in Huinan, Jilin Province, place deionized water, after abundant vibration is cleaned, drain to be placed on and dry 5h in the electrically heated drying cabinet under 100 ℃, back mechanical crushing, it is standby to cross 200 mesh sieves.
(2) preparation 3.0% sodium alginate soln (mass percent):
In glass beaker, add the 500mL deionized water in advance, be placed on the electric mixer, under 50 ℃ of heating conditions, pour the 15.0g sodium alginate solid that is taken by weighing fast into, be stirred well to this solution clear with the 500r/min rotating speed, the air bubble that may exist in the solution is removed with 100% power ultrasonic 3min in the back.
(3) preparation of 0.05mol/L calcium chloride solution:
Accurately take by weighing 5.549g anhydrous calcium chloride solid in the 100mL glass beaker, add after an amount of secondary deionized water fully dissolves, being transferred to 1000mL volumetric flask constant volume, to obtain the 0.05mol/L calcium chloride solution standby.
(4) preparation scoria-sodium alginate suspension (scoria mass percent 3.74%, sodium alginate mass percent 2.80%):
Take by weighing pretreated scoria powder among the 8.0g (1), be added in 3.0% sodium alginate soln of being prepared among the 200mL (2), make that scoria and sodium alginate mass percent are respectively in the solution: 3.74%, 2.80%.After this mixed solution is placed on the magnetic stirrer, with the full and uniform stirring of high speed 30min, it is standby to obtain scoria-sodium alginate suspension.
(5) be cross-linked to form scoria-sodium alginate complex microsphere:
After prepared suspension is removed the air bubble that wherein may exist with 100% power ultrasonic 3min in (4), scoria-sodium alginate suspension is passed through peristaltic pump, under the 2mL/min flow velocity, dropwise splash into (this solution places the 500mL glass beaker) in the 200mL 0.05mol/L calcium chloride solution, the scoria-sodium alginate micro ball that is cross-linked to form is dispersed in the 500mL glass beaker.After make microballoon in former calcium chloride solution, leave standstill 12h so that this micro-sphere crosslinked reacting completely, with washed with de-ionized water thus obtained microsphere 3 times, be neutrality to the supernatant cleaning fluid after, filter standby.
(6) the dry scoria-sodium alginate complex microsphere of handling:
Place electrically heated drying cabinet, temperature to be set to 70 ℃ thus obtained microsphere tiling in above-mentioned (5), drying time, 20h made the complete dehydration of wet microballoon, and obtaining dry average grain diameter is scoria-sodium alginate complex microsphere of 1.5mm.
(7) the dry natural scoria-sodium alginate complex microsphere for preparing, as effective water body purification material, the absorption that is applied to phosphorus in the water is removed:
The chemical constituent of the natural scoria that present embodiment prepares-sodium alginate complex microsphere water body purification material is sodium alginate-supported body and volcanic ash, and its mass ratio is 3: 4; Wherein the molecular formula of sodium alginate is (C
6H
7NaO
6) n, pozzuolanic constituent content (mass percent) is: Fe 8.81%, Al 8.89%, Ti 1.37%, Ca 4.91%, Mg3.19%, K 1.67%, Na 3.22%, Si 21.10% and O 46.84%.The average grain diameter of prepared natural scoria-sodium alginate complex microsphere is 1.5mm.Prepared material natural scoria-sodium alginate complex microsphere pattern characterizes sees accompanying drawing 1.
Experiment is removed in the phosphorus absorption in water of prepared water body purification material application, test draws, and is in the 15mg/L potassium dihydrogen phosphate, at pH=3 in that the 1.5g material is dropped into the 10mL initial concentration, be oscillating reactions 7h on the shaking table of 200r/min at rotating speed, the clearance of phosphorus is 91.39%; Simultaneously, the static reaction clearance is 86.82% under the same conditions.
Embodiment 7
(1) natural scoria preprocessing process:
Take by weighing the regional natural scoria 0.5kg in Huinan, Jilin Province, place deionized water, after abundant vibration is cleaned, drain to be placed on and dry 5h in the electrically heated drying cabinet under 100 ℃, back mechanical crushing, it is standby to cross 200 mesh sieves.
(2) preparation 3.0% sodium alginate soln (mass percent):
In glass beaker, add the 500mL deionized water in advance, be placed on the electric mixer, under 50 ℃ of heating conditions, pour the 15.0g sodium alginate solid that is taken by weighing fast into, be stirred well to this solution clear with the 500r/min rotating speed, the air bubble that may exist in the solution is removed with 100% power ultrasonic 3min in the back.
(3) preparation of 0.2mol/L calcium chloride solution:
Accurately take by weighing 22.198g anhydrous calcium chloride solid in the 500mL glass beaker, add after an amount of secondary deionized water fully dissolves, being transferred to 1000mL volumetric flask constant volume, to obtain the 0.2mol/L calcium chloride solution standby.
(4) preparation scoria-sodium alginate suspension (scoria mass percent 3.74%, sodium alginate mass percent 2.80%):
Take by weighing pretreated scoria powder among the 8.0g (1), be added in 3.0% sodium alginate soln of being prepared among the 200mL (2), make that scoria and sodium alginate percentage by weight are respectively in the solution: 3.74%, 2.80%.After this mixed solution is placed on the magnetic stirrer, with the full and uniform stirring of high speed 30min, it is standby to obtain scoria-sodium alginate suspension.
(5) be cross-linked to form scoria-sodium alginate complex microsphere:
After prepared suspension is removed the air bubble that wherein may exist with 100% power ultrasonic 3min in (4), scoria-sodium alginate suspension is passed through peristaltic pump, under the 2mL/min flow velocity, dropwise splash into (this solution places the 500mL glass beaker) in the 200mL 0.2mol/L calcium chloride solution, the scoria-sodium alginate micro ball that is cross-linked to form is dispersed in the 500mL glass beaker.After make microballoon in former calcium chloride solution, leave standstill 12h so that this micro-sphere crosslinked reacting completely, with washed with de-ionized water thus obtained microsphere 3 times, be neutrality to the supernatant cleaning fluid after, filter standby.
(6) the dry scoria-sodium alginate complex microsphere of handling:
Place electrically heated drying cabinet, temperature to be set to 70 ℃ thus obtained microsphere tiling in above-mentioned (5), drying time, 20h made the complete dehydration of wet microballoon, and obtaining dry average grain diameter is scoria-sodium alginate complex microsphere of 1.5mm.
(7) the dry natural scoria-sodium alginate complex microsphere for preparing, as effective water body purification material, the absorption that is applied to phosphorus in the water is removed:
The chemical constituent of the natural scoria that present embodiment prepares-sodium alginate complex microsphere water body purification material is sodium alginate-supported body and volcanic ash, and its mass ratio is 3: 4; Wherein the molecular formula of sodium alginate is (C
6H
7NaO
6) n, pozzuolanic constituent content (mass percent) is: Fe 8.81%, Al 8.89%, Ti 1.37%, Ca 4.91%, Mg3.19%, K 1.67%, Na 3.22%, Si 21.10% and O 46.84%.The average grain diameter of prepared natural scoria-sodium alginate complex microsphere is 1.5mm.Prepared material natural scoria-sodium alginate complex microsphere pattern characterizes sees accompanying drawing 1.
Experiment is removed in the phosphorus absorption in water of prepared water body purification material application, and test draws, and is in the 15mg/L potassium dihydrogen phosphate in that the 1.5g material is dropped into the 10mL initial concentration, and at pH=3,200r/min oscillating reactions 7h, the clearance of phosphorus are 95.20%; Simultaneously, the static reaction clearance is 90.0% under the same conditions.
Embodiment 8
(1) natural scoria preprocessing process:
Take by weighing the regional natural scoria 0.5kg in Huinan, Jilin Province, place deionized water, after abundant vibration is cleaned, drain to be placed on and dry 5h in the electrically heated drying cabinet under 100 ℃, back mechanical crushing, it is standby to cross 200 mesh sieves.
(2) preparation 0.5% sodium alginate soln (mass percent):
In glass beaker, add the 500mL deionized water in advance, be placed on the electric mixer, under 50 ℃ of heating conditions, pour the 2.5g sodium alginate solid that is taken by weighing fast into, be stirred well to this solution clear with the 500r/min rotating speed, the air bubble that may exist in the solution is removed with 100% power ultrasonic 3min in the back.
(3) preparation of 1.5mol/L calcium chloride solution:
Accurately take by weighing 166.485g anhydrous calcium chloride solid in the 500mL glass beaker, add after an amount of secondary deionized water fully dissolves, being transferred to 1000mL volumetric flask constant volume, to obtain the 1.5mol/L calcium chloride solution standby.
(4) preparation scoria-sodium alginate suspension (scoria mass percent 2.90%, sodium alginate mass percent 0.48%):
Take by weighing pretreated scoria powder among the 6.0g (1), be added in 0.5% sodium alginate soln of being prepared among the 200mL (2), make that scoria and sodium alginate mass percent are respectively in the solution: 2.90%, 0.48%.After this mixed solution is placed on the magnetic stirrer, with the full and uniform stirring of high speed 30min, it is standby to obtain scoria-sodium alginate suspension.
(5) be cross-linked to form scoria-sodium alginate complex microsphere:
After prepared suspension is removed the air bubble that wherein may exist with 100% power ultrasonic 3min in (4), scoria-sodium alginate suspension is passed through peristaltic pump, under the 2mL/min flow velocity, dropwise splash into (this solution places the 500mL glass beaker) in the 200mL 1.5mol/L calcium chloride solution, the scoria-sodium alginate micro ball that is cross-linked to form is dispersed in the 500mL glass beaker.After make microballoon in former calcium chloride solution, leave standstill 12h so that this micro-sphere crosslinked reacting completely, with washed with de-ionized water thus obtained microsphere 3 times, be neutrality to the supernatant cleaning fluid after, filter standby.
(6) the dry scoria-sodium alginate complex microsphere of handling:
Place electrically heated drying cabinet, temperature to be set to 70 ℃ thus obtained microsphere tiling in above-mentioned (5), drying time, 20h made the complete dehydration of wet microballoon, and obtaining dry average grain diameter is scoria-sodium alginate complex microsphere of 0.5～1.0mm.
(7) the dry natural scoria-sodium alginate complex microsphere for preparing, as effective water body purification material, the absorption that is applied to phosphorus in the water is removed:
The chemical constituent of the natural scoria that present embodiment prepares-sodium alginate complex microsphere water body purification material is sodium alginate-supported body and volcanic ash, and its mass ratio is 1: 6; Wherein the molecular formula of sodium alginate is (C
6H
7NaO
6) n, pozzuolanic constituent content (mass percent) is: Fe 8.81%, Al 8.89%, Ti 1.37%, Ca 4.91%, Mg3.19%, K 1.67%, Na 3.22%, Si 21.10% and O 46.84%.The average grain diameter of prepared natural scoria-sodium alginate complex microsphere is 0.5～1.0mm.Prepared material natural scoria-sodium alginate complex microsphere pattern characterizes sees accompanying drawing 1.
Experiment is removed in the phosphorus absorption in water of prepared water body purification material application, test draws, and is in the 15mg/L potassium dihydrogen phosphate, at pH=3 in that the 3g material is dropped into the 10mL initial concentration, be oscillating reactions 7h on the shaking table of 200r/min at rotating speed, the clearance of phosphorus is 86.52%; Simultaneously, the static reaction clearance is 78.30% under the same conditions.
Embodiment 9
(1) natural scoria preprocessing process:
Take by weighing the regional natural scoria 0.5kg in Huinan, Jilin Province, place deionized water, after abundant vibration is cleaned, drain to be placed on and dry 5h in the electrically heated drying cabinet under 100 ℃, back mechanical crushing, it is standby to cross 200 mesh sieves.
(2) preparation 3.0% sodium alginate soln (mass percent):
In glass beaker, add the 500mL deionized water in advance, be placed on the electric mixer, under 50 ℃ of heating conditions, pour the 15.0g sodium alginate solid that is taken by weighing fast into, be stirred well to this solution clear with the 500r/min rotating speed, the air bubble that may exist in the solution is removed with 100% power ultrasonic 3min in the back.
(3) preparation of 1.5mol/L calcium chloride solution:
Accurately take by weighing 166.485g anhydrous calcium chloride solid in the 500mL glass beaker, add after an amount of secondary deionized water fully dissolves, being transferred to 1000mL volumetric flask constant volume, to obtain the 1.5mol/L calcium chloride solution standby.
(4) preparation scoria-sodium alginate suspension (scoria mass percent 3.74%, sodium alginate mass percent 2.80%):
Take by weighing pretreated scoria powder among the 8.0g (1), be added in 3.0% sodium alginate soln of being prepared among the 200mL (2), make that scoria and sodium alginate mass percent are respectively in the solution: 3.74%, 2.80%.After this mixed solution is placed on the magnetic stirrer, with the full and uniform stirring of high speed 30min, it is standby to obtain scoria-sodium alginate suspension.
(5) be cross-linked to form scoria-sodium alginate complex microsphere:
After prepared suspension is removed the air bubble that wherein may exist with 100% power ultrasonic 3min in (4), scoria-sodium alginate suspension is passed through peristaltic pump, under the 2mL/min flow velocity, dropwise splash into (this solution places the 500mL glass beaker) in the 200mL 1.5mol/L calcium chloride solution, the scoria-sodium alginate micro ball that is cross-linked to form is dispersed in the 500mL glass beaker.After make microballoon in former calcium chloride solution, leave standstill 12h so that this micro-sphere crosslinked reacting completely, with washed with de-ionized water thus obtained microsphere 3 times, be neutrality to the supernatant cleaning fluid after, filter standby.
(6) the dry scoria-sodium alginate complex microsphere of handling:
Place electrically heated drying cabinet, temperature to be set to 70 ℃ thus obtained microsphere tiling in above-mentioned (5), drying time, 20h made the complete dehydration of wet microballoon, and obtaining dry average grain diameter is scoria-sodium alginate complex microsphere of 1.5～2.0mm.
(7) the dry natural scoria-sodium alginate complex microsphere for preparing, as effective water body purification material, the absorption that is applied to phosphorus in the water is removed:
The chemical constituent of the natural scoria that present embodiment prepares-sodium alginate complex microsphere water body purification material is sodium alginate-supported body and volcanic ash, and its mass ratio is 3: 4; Wherein the molecular formula of sodium alginate is (C
6H
7NaO
6) n, pozzuolanic constituent content (mass percent) is: Fe 8.81%, Al 8.89%, Ti 1.37%, Ca 4.91%, Mg3.19%, K 1.67%, Na 3.22%, Si 21.10% and O 46.84%.The average grain diameter of prepared natural scoria-sodium alginate complex microsphere is 1.5～2.0mm.Prepared material natural scoria-sodium alginate complex microsphere pattern characterizes sees accompanying drawing 1.
Experiment is removed in the phosphorus absorption in water of prepared water body purification material application, test draws, and is in the 15mg/L potassium dihydrogen phosphate, at pH=3 in that the 1.5g material is dropped into the 10mL initial concentration, be oscillating reactions 7h on the shaking table of 200r/min at rotating speed, the clearance of phosphorus is 92.20%; Simultaneously, the static reaction clearance is 85.43% under the same conditions.
Claims (10)
1. natural scoria-sodium alginate complex microsphere water body purification preparation methods, it is characterized in that, obtain dropwise splashing in the calcium chloride solution behind scoria-sodium alginate suspension solution by natural scoria being scattered in sodium alginate soln, be cross-linked to form scoria-sodium alginate complex microsphere drying or directly as the water body purification material.
2. natural scoria according to claim 1-sodium alginate complex microsphere water body purification preparation methods is characterized in that, described natural scoria through vibration cleaning and grain diameter is: below 200 orders.
3. natural scoria according to claim 1-sodium alginate complex microsphere water body purification preparation methods is characterized in that the concentration of described sodium alginate soln is: 0.5-3.0wt%.
4. natural scoria according to claim 1-sodium alginate complex microsphere water body purification preparation methods is characterized in that the concentration of described calcium chloride solution is: 0.05-1.5mol/L.
5. natural scoria according to claim 1-sodium alginate complex microsphere water body purification preparation methods, it is characterized in that, described dispersion is meant: behind the ratio adding sodium alginate soln of natural scoria with 30-40g/1L, adopt magnetic stirrer evenly to stir and the ultrasonic air bubble of removing wherein.
6. natural scoria according to claim 1-sodium alginate complex microsphere water body purification preparation methods, it is characterized in that described drying is meant: scoria-sodium alginate complex microsphere tiling is placed electrically heated drying cabinet dry 20h under 70 ℃ of environment.
7. the natural scoria for preparing according to the described method of above-mentioned arbitrary claim-sodium alginate complex microsphere water body purification material.
8. the natural scoria that the obtains-sodium alginate complex microsphere water body purification material according to the described method preparation of above-mentioned arbitrary claim is characterized in that its component is sodium alginate-supported body and volcanic ash, and mass ratio is 1: 8～1: 1; Wherein the molecular formula of sodium alginate is (C
6H
7NaO
6)
n, the content of pozzuolanic element and mass percent are: Fe 8.81%, Al 8.89%, Ti 1.37%, Ca 4.91%, Mg3.19%, K 1.67%, Na 3.22%, Si 21.10% and O 46.84%.
9. natural scoria according to claim 8-sodium alginate complex microsphere water body purification material is characterized in that described scavenging material is the complex microsphere structure, and average grain diameter is 0.5～3.0mm.
10. the application according to the described natural scoria of above-mentioned arbitrary claim-sodium alginate complex microsphere water body purification material is characterized in that, removes pollutant in the water body by described water body purification material being added Yu Shuizhong absorption.
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| CN102671641A (en) * | 2012-05-24 | 2012-09-19 | 上海交通大学 | Preparation and application for nanometer SiO2 strengthened calcium alginate-xanthan gum composite absorbent |
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| EP2733119A1 (en) * | 2012-11-20 | 2014-05-21 | Zachodniopomorski Uniwersytet Technologiczny w Szczecinie | Agent for removing dissolved phosphorus compounds from water |
| CN104959132A (en) * | 2015-06-16 | 2015-10-07 | 昆明理工大学 | Preparation method of carbon dioxide calcium-based adsorbent |
| CN105498695A (en) * | 2015-12-02 | 2016-04-20 | 南京师范大学 | Sodium alginate-MOF (metal organic framework) composite spherule as well as preparation method and application thereof |
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| CN102476039A (en) * | 2010-11-27 | 2012-05-30 | 中国科学院兰州化学物理研究所 | Method for preparing composite microsphere drying agent |
| CN102671614A (en) * | 2012-04-24 | 2012-09-19 | 中国环境科学研究院 | Double-metal macromolecule permeable reactive barrier stuffing material and preparation method thereof |
| CN102671641A (en) * | 2012-05-24 | 2012-09-19 | 上海交通大学 | Preparation and application for nanometer SiO2 strengthened calcium alginate-xanthan gum composite absorbent |
| EP2732872A1 (en) * | 2012-11-20 | 2014-05-21 | Zachodniopomorski Uniwersytet Technologiczny w Szczecinie | Method of producing agent for removing dissolved phosphorus compounds from water and agent for removing dissolved phosphorus compounds from water |
| EP2733119A1 (en) * | 2012-11-20 | 2014-05-21 | Zachodniopomorski Uniwersytet Technologiczny w Szczecinie | Agent for removing dissolved phosphorus compounds from water |
| CN104959132A (en) * | 2015-06-16 | 2015-10-07 | 昆明理工大学 | Preparation method of carbon dioxide calcium-based adsorbent |
| CN105498695A (en) * | 2015-12-02 | 2016-04-20 | 南京师范大学 | Sodium alginate-MOF (metal organic framework) composite spherule as well as preparation method and application thereof |
| CN107694533A (en) * | 2017-08-03 | 2018-02-16 | 天津大学 | A kind of polypyrrole load volcanic ash compound adsorbent and preparation method and application |
| CN108927117A (en) * | 2018-08-02 | 2018-12-04 | 深圳市深港产学研环保工程技术股份有限公司 | A kind of preparation method of flyash-sodium alginate composite adsorbing material |
| CN111170432A (en) * | 2020-01-14 | 2020-05-19 | 龙岩绿合环保有限公司 | Moisture-proof water purifying agent and preparation method and use method thereof |
| CN115869917A (en) * | 2022-11-30 | 2023-03-31 | 东华大学 | Preparation method of calcium alginate microspheres |
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